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tert-butyl N-(4-aminobutyl)carbamate → HCID 86626162, 화합물

HRID 598318
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HRID 598318 반응식
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[N:15]=[CH:14][C:13]([N+:19]([O-:21])=[O:20])=[C:12]2Cl)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[NH2:30][CH2:31][CH2:32][CH2:33][CH2:34][NH:35][C:36](=[O:42])[O:37][C:38]([CH3:41])([CH3:40])[CH3:39]>ClCCl.NCCCCNC(=O)OC(C)(C)C>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[N:15]=[CH:14][C:13]([N+:19]([O-:21])=[O:20])=[C:12]2[NH:30][CH2:31][CH2:32][CH2:33][CH2:34][NH:35][C:36](=[O:42])[O:37][C:38]([CH3:40])([CH3:39])[CH3:41])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 4351tert-butyl N-(4-aminobutyl)carbamateHCID 8471TriethylamineHCID 670509926-(Benzyloxy)-4-chloro-3-nitroquinoline

생성물 1

HCID 86626162HCID 86626162, 화합물수율 81.6%

시약·촉매·용매 2

HCID 4351tert-butyl N-(4-aminobutyl)carbamate촉매
HCID 6344
Dichloromethane
용매

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온도
0 °C

실험 절차

A solution of 6-benzyloxy-4-chloro-3-nitroquinoline (14.47 g, 46.29 mmol), prepared in Parts A-D of Example 57, and triethylamine (8.4 mL, 60.2 mmol) in dichloromethane (200 mL) was cooled to 0° C. tert-Butyl N-(4-aminobutyl)carbamate (8.71 g, 46.3 mmol) was added; the reaction was stirred for 15 minutes at 0° C. and then allowed to warm to ambient temperature and stirred for five hours. An analysis by TLC indicated the presence of starting material; therefore, additional tert-butyl N-(4-aminobutyl)carbamate (0.5 mL, 2.6 mmol) was added. The reaction was stirred overnight and then washed with water (2×200 mL). The combined washings were extracted with chloroform after the addition of sodium chloride. The combined organic solutions were dried over sodium sulfate, filtered, and concentrated under reduced pressure. The crude product was recrystallized from ethyl acetate (100 mL). The crystals were isolated by filtration and washed with cold hexanes to provide 17.62 g of tert-butyl [4-(6-benzyloxy-3-nitroquinolin-4-ylamino)butyl]carbamate as an orange powder.

후처리

  1. additionwas added
  2. temperatureto warm to ambient temperature
  3. stirringstirred for five hours
  4. stirringThe reaction was stirred overnight
  5. washwashed with water (2×200 mL)
  6. extractionThe combined washings were extracted with chloroform
  7. additionafter the addition of sodium chloride
  8. dry with materialThe combined organic solutions were dried over sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated under reduced pressure
  11. customThe crude product was recrystallized from ethyl acetate (100 mL)
  12. customThe crystals were isolated by filtration
  13. washwashed with cold hexanes

출처 및 근거

ORD 기록
ord-79e581bdd58a4389adfff60789a2f985
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07897597B2

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